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Processing and Martensitic Transformations of NiTi-based Alloys
Kuběnová, Monika ; Kroupa, Aleš (oponent) ; Zemčík, Ladislav (oponent) ; Dlouhý, Antonín (vedoucí práce)
The thesis aims at: (i) an assessment of alloy contamination which may result from vacuum induction melting of Ni-rich NiTi-based shape memory alloys in conventional porous Y2O3 crucibles. (ii) an optimization of NiTi melting conditions with respect to the alloy purity and cost efficiency. (iii) an obtaining new differential scanning calorimetry (DSC) and 3D atom probe (AP) data on martensitic transformations and related hydrogen distributions in the Ni-rich NiTi shape memory alloys subjected to heat treatments under controlled environments with systematic variation of the hydrogen partial pressure. The following experiments were carried out: – Five different melting routes were designed and carried out in order to decrease melting temperature. – Five re-melting experiments were performed at 1500 °C with holding time 2, 10 and 20 min, and at 1550 °C and 1450 °C with 20 min holding time to examine the effect of temperature and holding time on oxygen content. – Ni-rich NiTi alloys were heat treated in Regime I (annealing) and in Regime II (annealing and aging) in either hydrogen or hydrogen-helium mixture (H2 partial pressure 20, 100, 500 and 700 mbar). Reference experiment were also performed in a pure helium atmosphere. It was found that designed melting routes lead to the lowering of maximum temperature during the induction melting cycles from 1800 to 1400 °C. Despite this significant maximum temperature drop, oxygen content of the final solidified alloy does not markedly reduce. During re-melting at 1500 °C with 2 min of holding time, the content of oxygen becomes triple the initial oxygen level and does not too differ from the re-melting experiments carried out at the same melting temperature but with 10 min of holding time. Furthermore, the oxygen content increases about fourfold with respect to the initial oxygen level during re-melting for 20 min at 1450 °C. This contamination level does not vary markedly with further rise of the melting temperature by 100 °C. Heat treatments in the controlled gaseous environments revealed that the one-step B2-B19’ martensitic transformation ceases with the increasing partial pressure of hydrogen. A pronounced drop in the DSC peak heights occurs at the hydrogen partial pressure exceeding 100 mbar. 3D AP measurements showed that there are no local variations in the Ni and Ti compositions in the sample after the Regime I heat treatment in hydrogen. Hydrogen was found to form stable interstitial solid solution in B2 NiTi. The distribution of hydrogen atoms is inhomogeneous; they organize into nano-domains with the hydrogen content exceeding locally a level of 10 at%.
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Hodnocení homogenity ingotů slitiny Ni-Ti metodou DSC
Kuběnová, Monika ; Zemčík, Ladislav (oponent) ; Dlouhý, Antonín (vedoucí práce)
Sliitny NiTi o blízkém ekviatomárním složení niklu a titianu patří do skupiny materiálů, které vykazují tvarovou paměť. Slitiny NiTi jsou velmi atraktivní funkční materiály a to nejen diky své tvarové paměti s vysokou pevností, houževnatostí, ale i svými unikátními fyzikálními vlastnostmi. Výroba těchto slitin je velmi obtížná. Striktním požadavkem na výrobu těchto slitin je dodržení chemického složení, které spolu s tepleně-mechanickými úpravami výrazně ovlivňují výsledné vlastnosti slitiny. Tato práce je zaměřena na hodnocení homogenity ingotu slitiny NiTi o nominálním složení 50,8 at.% Ni, který byl připraven vakuovým indukčním tavením v Y203 kelímku. Hodnocení homogenity se opírá zajména o metodu DSC. V práci jsou korelovány DSC výsledky s mikrostrukturou slitiny, která byla analyzována metodmami SEM a TEM.
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AN INTERPLAY BETWEEN HEAT TREATMENT CONDITIONS AND B2 <-> B19 ' TRANSFORMATION IN Ni-Ti SHAPE MEMORY ALLOYS
Kuběnová, Monika ; Zálešák, Jakub ; Čermák, Jiří ; Dlouhý, Antonín
This study investigates the influence of a heat treatment atmosphere on multistage martensitic transformations in a Ti-50.9at% Ni shape memory alloy. Evacuated quartz tubes were filled with hydrogen while the hydrogen partial pressure was carefully controlled in each experiment. The encapsulated specimens were subjected to heat treatments consisting of annealing and aging. After the heat treatment, the path of martensitic transformation was investigated using differential scanning calorimetry (DSC). On cooling, martensite initial temperatures decrease with the increasing partial pressure of hydrogen applied during the heat treatment. Moreover, the formation of martensite phase may not take place for partial pressures that exceed a certain limit. On the other hand, two-and multiple-step B2/R/B19' martensitic transformations are observed in specimens heat treated at lower hydrogen pressures. Results obtained using transmission electron microscopy (TEM) clearly show that the size of Ni4Ti3 precipitates becomes smaller in alloys that were heat treated at higher hydrogen pressures. The results are discussed in terms of a chain of events. It is suggested that diffusion of hydrogen into the specimen during the annealing step first influences the nucleation of the Ni4Ti3 phase. The sizes and distribution of the Ni4Ti3 precipitates than control the characteristics of B2/B19' transformation.
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Processing and Martensitic Transformations of NiTi-based Alloys
Kuběnová, Monika ; Kroupa, Aleš (oponent) ; Zemčík, Ladislav (oponent) ; Dlouhý, Antonín (vedoucí práce)
The thesis aims at: (i) an assessment of alloy contamination which may result from vacuum induction melting of Ni-rich NiTi-based shape memory alloys in conventional porous Y2O3 crucibles. (ii) an optimization of NiTi melting conditions with respect to the alloy purity and cost efficiency. (iii) an obtaining new differential scanning calorimetry (DSC) and 3D atom probe (AP) data on martensitic transformations and related hydrogen distributions in the Ni-rich NiTi shape memory alloys subjected to heat treatments under controlled environments with systematic variation of the hydrogen partial pressure. The following experiments were carried out: – Five different melting routes were designed and carried out in order to decrease melting temperature. – Five re-melting experiments were performed at 1500 °C with holding time 2, 10 and 20 min, and at 1550 °C and 1450 °C with 20 min holding time to examine the effect of temperature and holding time on oxygen content. – Ni-rich NiTi alloys were heat treated in Regime I (annealing) and in Regime II (annealing and aging) in either hydrogen or hydrogen-helium mixture (H2 partial pressure 20, 100, 500 and 700 mbar). Reference experiment were also performed in a pure helium atmosphere. It was found that designed melting routes lead to the lowering of maximum temperature during the induction melting cycles from 1800 to 1400 °C. Despite this significant maximum temperature drop, oxygen content of the final solidified alloy does not markedly reduce. During re-melting at 1500 °C with 2 min of holding time, the content of oxygen becomes triple the initial oxygen level and does not too differ from the re-melting experiments carried out at the same melting temperature but with 10 min of holding time. Furthermore, the oxygen content increases about fourfold with respect to the initial oxygen level during re-melting for 20 min at 1450 °C. This contamination level does not vary markedly with further rise of the melting temperature by 100 °C. Heat treatments in the controlled gaseous environments revealed that the one-step B2-B19’ martensitic transformation ceases with the increasing partial pressure of hydrogen. A pronounced drop in the DSC peak heights occurs at the hydrogen partial pressure exceeding 100 mbar. 3D AP measurements showed that there are no local variations in the Ni and Ti compositions in the sample after the Regime I heat treatment in hydrogen. Hydrogen was found to form stable interstitial solid solution in B2 NiTi. The distribution of hydrogen atoms is inhomogeneous; they organize into nano-domains with the hydrogen content exceeding locally a level of 10 at%.
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Hodnocení homogenity ingotů slitiny Ni-Ti metodou DSC
Kuběnová, Monika ; Zemčík, Ladislav (oponent) ; Dlouhý, Antonín (vedoucí práce)
Sliitny NiTi o blízkém ekviatomárním složení niklu a titianu patří do skupiny materiálů, které vykazují tvarovou paměť. Slitiny NiTi jsou velmi atraktivní funkční materiály a to nejen diky své tvarové paměti s vysokou pevností, houževnatostí, ale i svými unikátními fyzikálními vlastnostmi. Výroba těchto slitin je velmi obtížná. Striktním požadavkem na výrobu těchto slitin je dodržení chemického složení, které spolu s tepleně-mechanickými úpravami výrazně ovlivňují výsledné vlastnosti slitiny. Tato práce je zaměřena na hodnocení homogenity ingotu slitiny NiTi o nominálním složení 50,8 at.% Ni, který byl připraven vakuovým indukčním tavením v Y203 kelímku. Hodnocení homogenity se opírá zajména o metodu DSC. V práci jsou korelovány DSC výsledky s mikrostrukturou slitiny, která byla analyzována metodmami SEM a TEM.
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Microstructure Characterization and Faigue Behavior of Beta Phase Containing Gama-TiAl Alloy
Petrenec, Martin ; Beran, Přemysl ; Šmíd, Miroslav ; Chlupová, Alice ; Kuběnová, Monika
The microstructure and fatigue properties of Ti–44Al–7.8Nb – 0.2Ni (at.%) alloy after graded cooling heat treatment were investigated. Different techniques as SEM, TEM and FIB were used for characterization of microstructure. Quantification of phase volume fraction was measured by neutron diffraction method. After graded cooling heat treatment the structure consists of fully lamellar uniform grains which contain lamellar phases /2 and cubic phases (ordered B2 and disordered phases) at grain boundary and interlamellar spaces. The foils for TEM were prepared using FIB technique and observed in TEM in order to identify B2 phase by selected electron diffraction. Low cycle fatigue behaviour at 750 °C shows stable fatigue crack propagation due the presence of plastic beta and B2 phases.
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Impact of Heat Treatment Environment of Microstructure and Transformation Path in NiTi Shape Memory Alloy
Kuběnová, Monika ; Zálešák, Jakub ; Čermák, Jiří ; Barták, Tomáš ; Dlouhý, Antonín
We report results of differential scanning calorimetry (DSC) experiments in which heat flow (T) from and to Ti-50.9at%Ni shape memory samples was recorded during the temperature scan through a B2 B19’ transformation range. Prior to the DSC experiments, the samples were separately annealed in evacuated quartz capsules containing different hydrogen and helium mixtures with an overall filling pressure of 900 mbar. The quartz tubes containing the annealed samples were subsequently quenched into cold water. After quenching, the capsules were opened, martensitic transformations were investigated by DSC and the microstructure of the samples was assessed by transmission electron microscopy (TEM). Annealing in the mixtures with an increasing partial pressure of hydrogen led to a considerable drop in the latent heat associated with the B2 B19’ martensitic transformation. Results obtained using TEM suggest that hydrogen may function as a catalytic substance that accelerates the long range ordering of Ni atoms in early stages of Ni4Ti3-phase precipitation. The selected area diffraction study focused on patterns in <100>B2 and <110>B2 zones and provided evidence for diffuse scattering due to spatial modulations of the lattice constant. These variations in the background electron intensities might be related to a precursor of Ni4Ti3 phase in its early state of formation.
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Influence of Heat Treatment on Microstructure and Transformation Characteristics of NiTi Shape Memory Wires
Zálešák, Jakub ; Kuběnová, Monika ; Čermák, Jiří ; Svoboda, Milan ; Dlouhý, Antonín
The present study shows how heat treatments affect microstructure and transformation behaviour of superelastic Ni-rich NiTi shape memory wires. Wire samples were sealed into quartz tubes, filled with hydrogen reduction atmosphere, heated for 10 minutes at temperatures increasing in a range from 500 to 600°C and subsequently quenched into cold water. Characteristic transformation temperatures MS, MF, AS, AF, thermal hysteresis and latent heats were investigated using differential scanning calorimetry (DSC). We observed significant changes in DSC charts which recorded B2 → R and R → B19‘ phase martensitic transformations. Increasing temperature of the heat treatment resulted in a convergence of the two transformation peaks. R-transformation commenced at systematically lower temperatures and the beginning of the B19‘ transformation was shifted to higher temperatures with increasing temperature of the heat treatment. In parallel, latent heat of the overall B2 → B19‘ transformation clearly increases. We rationalize these significant changes in the transformation behaviour on the basis of the microstructural development during the heat treatment which is characterized by means of SEM, TEM and EBSD techniques.
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